Determination of potassium and sodium in vanadium-titanium-iron concentrate by microwave digestion-inductively coupled plasma atomic emission spectrometry
HUO Hong-ying
State Key Laboratory for Vanadium & Titanium Testing Panzhihua University, Panzhihua 617000, China
Abstract：The sample was treated in hydrochloric acid-hydrofluoric acid-water system by microwave digestion method. K 769.896 nm and Na 588.995 nm were selected as the analytical lines. A determination method of potassium and sodium in vanadium-titanium-iron concentrate was established by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results showed that 0.500 0 g of vanadium-titanium-iron concentrate sample could be completely dissolved by microwave digestion with 8.0 mL of hydrochloric acid, 5.0 mL of hydrofluoric acid and 5.0 mL of water. The iron matrix did not have influence on determination of sodium, but have great influence on determination of potassium which could not be ignored. The iron matrix solution which was roughly equivalent to that in test sample was added to standard solution series for calibration curves to eliminate the influence of iron matrix effect. The mass fraction of potassium and sodium in range of 0.006%-0.08% and 0.005%-0.04% were linear to their corresponding emission intensity with linear correlation coefficients of 0.999 8 and 0.999 9, respectively. The detection limit of potassium and sodium was 0.03% and 0.02%, respectively. The proposed method was applied to the determination of potassium and sodium in certified reference material of vanadium-titanium-iron concentrate, and the results were consistent with the certified values. The relative standard deviations (RSD, n=10) were less than 5%.
张磊,王晓艳,李波.微波消解技术在金属分析中的应用[J].光谱实验室,2010,27(3):953-957.ZHANG Lei,WANG Xiao-yan,LI Bo.Application of microwave digestion technology in metal analysis[J].Chinese Journal of Spectroscopy Laboratory,2010,27(3):953-957.
[5]
梁丽虹.ICP-AES法测定铁矿石中微量氧化钾、氧化钠[J].冶金丛刊,2004(2):14-15.LIANG Li-hong.ICP-AES to measure the trace element K2O and Na2O in iron ore[J].Metallurgical Collections,2004(2):14-15.
孙喜顺,王彦茹,阎雪,等.电感耦合等离子体原子发射光谱法测定钒钛铁精矿中的钒钛铝镁锰[J].冶金分析,2011,31(8):79-82.SUN Xi-shun,WANG Yan-ru,YAN Xue,et al.Determination of vanadium,titanium,aluminium,magnesium and manganese in vanadium-titanium-iron concentrate by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2011,31(8):79-82.
[8]
孙喜顺,王彦茹,安贵明,等.微波消解-电感耦合等离子体原子发射光谱法测定钒钛烧结矿中9种元素[J].冶金分析,2015,35(2):65-69.SUN Xi-shun,WANG Yan-ru,AN Gui-ming,et al.Microwave digestion-inductively coupled plasma atomic emission spectrometry for the determination of nine elements in vanadium-titanium sinter[J].Metallurgical Analysis,2015,35(2):65-69.
[9]
刘松利,白晨光,胡途,等.钒钛铁精矿内配碳球团高温快速直接还原历程[J].重庆大学学报:自然科学版,2011,34(1):60-65.LIU Song-li,BAI Chen-guang,HU Tu,et al.Quick and direct reduction process of vanadium and titanium iron concentrate with carbon-containing pellets at high temperature[J].Journal of Chongqing University:Natural Science Edition,2011,34(1):60-65.
